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WO2017208667A1 - Liquide de polissage et procédé de polissage chimico-mécanique - Google Patents

Liquide de polissage et procédé de polissage chimico-mécanique Download PDF

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Publication number
WO2017208667A1
WO2017208667A1 PCT/JP2017/015979 JP2017015979W WO2017208667A1 WO 2017208667 A1 WO2017208667 A1 WO 2017208667A1 JP 2017015979 W JP2017015979 W JP 2017015979W WO 2017208667 A1 WO2017208667 A1 WO 2017208667A1
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WIPO (PCT)
Prior art keywords
polishing liquid
polishing
group
mass
content
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2017/015979
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English (en)
Japanese (ja)
Inventor
上村　哲也
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Fujifilm Corp
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Fujifilm Corp
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Filing date
Publication date
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Priority to JP2018520714A priority Critical patent/JP6652638B2/ja
Priority to KR1020187033523A priority patent/KR102298238B1/ko
Publication of WO2017208667A1 publication Critical patent/WO2017208667A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09G—POLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00—Polishing compositions
    • C09G1/02—Polishing compositions containing abrasives or grinding agents
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • C09K3/1409—Abrasive particles per se
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • C09K3/1454—Abrasive powders, suspensions and pastes for polishing
    • H10P52/00—
    • H10P95/04—

Definitions

  • the present invention relates to a polishing liquid and a chemical mechanical polishing method.
  • CMP chemical mechanical polishing
  • a polishing liquid used in CMP for example, Patent Document 1 discloses a polishing characterized by containing “alcohol, abrasive grains, and water whose solubility in water is 0.5 to 8 wt% at a liquid temperature of 25 degrees. Liquid ".
  • the inventor examined the polishing liquid described in Patent Document 1 and found that there was a problem that the abrasive grains contained in the polishing liquid were likely to aggregate when the polishing liquid was stored. It has also been clarified that when the polishing liquid is applied to CMP, defects are likely to occur on the polished surface of the object to be polished.
  • the present invention is difficult to agglomerate abrasive grains (in other words, “having excellent stability over time”), and even when applied to CMP, defects (in other words, “scratch”) are present on the surface to be polished. It is an object of the present invention to provide a polishing liquid that does not easily occur. Another object of the present invention is to provide a chemical mechanical polishing method.
  • the present inventor is a polishing solution for chemical mechanical polishing containing abrasive grains, an organic acid, and a predetermined alcohol A, which contains alcohol A.
  • the present inventors have found that a polishing liquid whose amount is within a predetermined range can solve the above-mentioned problems, and completed the present invention. That is, it has been found that the above-described problem can be achieved by the following configuration.
  • a polishing liquid for chemical mechanical polishing containing abrasive grains, an organic acid, and alcohol A, wherein alcohol A is selected from the group consisting of methanol, ethanol, 1-propanol, and isopropanol.
  • a charge control agent is contained, and the charge control agent contains at least one selected from the group consisting of inorganic acids, ammonium salts of organic acids, and ammonium salts of inorganic acids, [1] or The polishing liquid according to [2].
  • the amino acids are glycine, alanine, arginine, isoleucine, leucine, valine, phenylalanine, asparagine, glutamine, lysine, histidine, proline, tryptophan, aspartic acid, glutamic acid, serine, threonine, tyrosine, cysteine, methionine, and N-.
  • the polishing liquid according to [6] which is at least one selected from the group consisting of methylglycine.
  • the polishing liquid according to [6] or [7] which contains two or more amino acids.
  • the azole compound different from the benzotriazole compound is at least one selected from the group consisting of 1,2,4-triazole compounds, pyrazole compounds, and imidazole compounds.
  • a polishing liquid which has excellent temporal stability and hardly causes defects on the surface to be polished even when applied to CMP (hereinafter also referred to as “having the effect of the present invention”). can do.
  • the present invention can also provide a chemical mechanical polishing method.
  • a numerical range expressed using “to” means a range including numerical values described before and after “to” as a lower limit value and an upper limit value.
  • a polishing liquid according to an embodiment of the present invention is a polishing liquid for chemical mechanical polishing containing abrasive grains, an organic acid, and an alcohol A, where the alcohol A is methanol, ethanol, 1 A polishing liquid which is at least one selected from the group consisting of propanol and isopropanol, and the content of alcohol A is 1.0 to 800 ppm by mass in the total mass of the polishing liquid.
  • ppm intends parts per million.
  • Alcohol A (Alc) One of the characteristic points of the polishing liquid is that the content of alcohol A is 1.0 to 800 ppm by mass in the total mass of the polishing liquid. If the content of alcohol A exceeds the upper limit, the absolute value of the zeta potential on the surface of the abrasive grains (particularly the surface of colloidal silica) decreases, and the abrasive grains tend to aggregate in the polishing liquid during storage. Is estimated to decrease. On the other hand, when the content of the alcohol A is less than the lower limit, when the polishing liquid is applied to CMP, defects are likely to occur on the surface to be polished of the object to be polished.
  • the content of the alcohol A is 1.0 to 800 ppm by mass, preferably 1.0 to 750 ppm by mass, and more preferably 10 to 500 ppm by mass with respect to the total mass of the polishing liquid.
  • the alcohol A is at least one selected from the group consisting of methanol, ethanol, 1-propanol, and isopropanol.
  • 1 type may be used independently or 2 or more types may be used together.
  • the total content of the two or more alcohols A is 1.0 to 800 ppm by mass, and the preferred range is as described above.
  • the content of alcohol A in the polishing liquid is intended to be the content measured by the following method.
  • the alcohol A content in the polishing liquid is measured using gas chromatography.
  • the measurement conditions for gas chromatography are as follows.
  • alcohol A content can be calculated
  • the pH of the polishing liquid is not particularly limited, but is usually 1.0 to 14.0. Of these, 5.0 to 8.0 is more preferable. When the pH is 5.0 or more, a polishing liquid having better stability over time can be obtained, and even when the polishing liquid is applied to CMP, defects on the surface to be polished are less likely to occur. Although the mechanism by which this effect is obtained is not necessarily clear, for example, since the isoelectric point of the zeta potential on the surface of the colloidal silica is around pH 4.0, the pH of the polishing liquid is within the above range above the isoelectric point. The present inventor presumes that the abrasive grains are less likely to aggregate by adjusting to. On the other hand, if the pH is 8.0 or less, dishing is less likely to occur on the surface to be polished of the object to be polished when the polishing liquid is applied to CMP.
  • the polishing liquid contains abrasive grains. It does not restrict
  • the abrasive grains include inorganic abrasive grains such as silica, alumina, zirconia, ceria, titania, germania, and silicon carbide; and organic abrasive grains such as polystyrene, polyacryl, and polyvinyl chloride.
  • silica particles are preferable as the abrasive grains in that the dispersion stability in the polishing liquid is excellent and the number of polishing scratches (scratches) generated by CMP is small.
  • the silica particles are not particularly limited, and examples thereof include precipitated silica, fumed silica, and colloidal silica. Of these, colloidal silica is more preferable.
  • the average primary particle diameter of the abrasive grains is not particularly limited, but is preferably 1 to 100 nm in that the polishing liquid has more excellent dispersion stability.
  • the average primary particle size can be confirmed by a manufacturer's catalog or the like.
  • Examples of commercially available abrasive grains include colloidal silica such as PL-1, PL-2, PL-3, PL-7, and PL-10H (all trade names are manufactured by Fuso Chemical Industries). It is done.
  • the content of the abrasive grains is not particularly limited, and is preferably 0.01% by mass or more, more preferably 0.1% by mass or more, and preferably 10% by mass or less, based on the total mass of the polishing liquid, and 5% by mass or less. Is more preferable. Within the above range, a more excellent polishing rate can be obtained when the polishing liquid is applied to CMP.
  • an abrasive grain may be used individually by 1 type, or may use 2 or more types together. When two or more kinds of abrasive grains are used in combination, the total content is preferably within the above range.
  • the content of the abrasive grains satisfies the following relationship with the content of the alcohol A. That is, the mass ratio of the alcohol A content to the abrasive content (alcohol A content / abrasive content; also referred to as “Alc / A” ratio) is 0.0001 to 1.5. Preferably, 0.01 to 0.08 is more preferable, and 0.1 to 0.7 is still more preferable. When the Alc / A ratio is 0.1 to 0.7, a better polishing rate can be obtained when the polishing liquid is applied to CMP.
  • the polishing liquid contains an organic acid.
  • the organic acid is a compound different from the oxidizing agent and charge adjusting agent described later, and has functions of promoting oxidation of the metal, adjusting the pH of the polishing liquid, and as a buffer.
  • As the organic acid a water-soluble organic acid is preferable. It does not restrict
  • organic acid examples include 1-hydroxyethylidene-1,1-diphosphonic acid (hereinafter also referred to as “HEDP”), diethylenetriaminepentaacetic acid (hereinafter also referred to as “DTPA”), formic acid, acetic acid, propionic acid, Butyric acid, valeric acid, 2-methylbutyric acid, n-hexanoic acid, 3,3-dimethylbutyric acid, 2-ethylbutyric acid, 4-methylpentanoic acid, n-heptanoic acid, 2-methylhexanoic acid, n-octanoic acid, 2 -Ethylhexanoic acid, benzoic acid, glycolic acid, salicylic acid, glyceric acid, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, maleic acid, phthalic acid, malic acid, tartaric acid, citric acid, lactic acid,
  • an amino acid is more preferable in that it has superior water solubility. It does not restrict
  • amino acids include glycine, alanine ( ⁇ -alanine and / or ⁇ -alanine), arginine, isoleucine, leucine, valine, phenylalanine, asparagine, glutamine, lysine, histidine, proline, tryptophan, aspartic acid, glutamic acid, serine, Examples include threonine, tyrosine, cysteine, methionine, and N-methylglycine.
  • glycine, ⁇ -alanine, ⁇ -alanine, L-aspartic acid, or methylglycine is preferable as the amino acid in that the polishing liquid has a more excellent effect of the present invention.
  • / or methylglycine is more preferred.
  • an amino acid may be used individually by 1 type, or may use 2 or more types together.
  • polishing liquid contains a 2 or more types of amino acid at the point from which the polishing liquid which has the effect of this invention more excellent is obtained.
  • the two or more amino acids are not particularly limited, and the above amino acids can be used in combination.
  • glycine and alanine are used as two or more amino acids in that a superior polishing rate is obtained when the polishing liquid is applied to CMP, and dishing is less likely to occur on the surface to be polished.
  • a combination of alanine and N-methylglycine or glycine and N-methylglycine is preferable.
  • the content of the organic acid is not particularly limited and is preferably 0.1% by mass or more, more preferably 0.5% by mass or more, still more preferably 1.0% by mass or more based on the total mass of the polishing liquid. 50 mass% or less is preferable, 25 mass% or less is more preferable, 20 mass% or less is further more preferable, and 10 mass% or less is especially preferable.
  • the content of the organic acid is 0.1% by mass or more, a more excellent polishing rate can be obtained when the polishing liquid is applied to CMP. Further, when the content of the organic acid is 50% by mass or less, dishing is less likely to occur on the surface to be polished when the polishing liquid is applied to CMP.
  • an organic acid may be used individually by 1 type, or may use 2 or more types together.
  • the total content is preferably within the above range.
  • the content of the organic acid preferably satisfies the following relationship with the content of the alcohol A. That is, the mass ratio of the alcohol A content to the organic acid content (alcohol A content / organic acid content; also referred to as “Alc / B” ratio) is 0.0001 to 0.2. Preferably, 0.0006 to 0.1 is more preferable, and 0.001 to 0.05 is still more preferable. When the Alc / B ratio is 0.001 to 0.05, a better polishing rate can be obtained when the polishing liquid is applied to CMP.
  • the polishing liquid may contain components other than the above as optional components. Below, an arbitrary component is demonstrated.
  • the polishing liquid may contain an anticorrosive agent. It is preferable that the anticorrosive agent has an action of controlling corrosion of the metal by adsorbing to the surface to be polished of the object to be polished to form a film.
  • the anticorrosive agent is not particularly limited, and a known anticorrosive agent can be used, and among them, an azole compound is preferable.
  • the azole compound means a compound containing a hetero five-membered ring containing one or more nitrogen atoms, and the number of nitrogen atoms is preferably 1 to 4.
  • the azole compound may contain atoms other than nitrogen atoms as heteroatoms.
  • guide_body intends the compound which has the substituent which the said heterocyclic 5-membered ring can contain.
  • the azole compound examples include pyrrole skeleton, imidazole skeleton, pyrazole skeleton, isothiazole skeleton, isoxazole skeleton, triazole skeleton, tetrazole skeleton, imidazole skeleton, thiazole skeleton, oxazole skeleton, isoxazole skeleton, thiadiazole skeleton, and oxadiazole. Examples thereof include compounds having a skeleton and a tetrazole skeleton.
  • the azole compound may be an azole compound containing a polycyclic structure containing a condensed ring in the skeleton.
  • Examples of the azole compound containing a polycyclic structure include compounds containing an indole skeleton, a purine skeleton, an indazole skeleton, a benzimidazole skeleton, a carbazole skeleton, a benzoxazole skeleton, a benzothiazole skeleton, a benzothiadiazole skeleton, and a naphthimidazole skeleton. Is mentioned.
  • the substituent that the azole compound may contain is not particularly limited, and examples thereof include a halogen atom (a fluorine atom, a chlorine atom, a bromine atom, or an iodine atom), an alkyl group (a linear, branched, or cyclic alkyl group, A polycyclic alkyl group such as an alkyl group or an active methine group may be included), an alkenyl group, an alkynyl group, an aryl group, a heterocyclic group (regarding the position of substitution), an acyl group, an alkoxycarbonyl group , Aryloxycarbonyl group, heterocyclic oxycarbonyl group, carbamoyl group (Examples of the carbamoyl group having a substituent include N-hydroxycarbamoyl group, N-acylcarbamoyl group, N-sulfonylcarbamoyl group, N-carbamoylcarbamoyl
  • a halogen atom (a fluorine atom, a chlorine atom, a bromine atom, or an iodine atom
  • an alkyl group (a linear, branched or cyclic alkyl group, even a polycyclic alkyl group such as a bicycloalkyl group, An active methine group may be included), an alkenyl group, an alkynyl group, an aryl group, or a heterocyclic group (regarding the position of substitution).
  • active methine group means a methine group substituted with two electron-attracting groups.
  • the “electron withdrawing group” is, for example, an acyl group, an alkoxycarbonyl group, an aryloxycarbonyl group, a carbamoyl group, an alkylsulfonyl group, an arylsulfonyl group, a sulfamoyl group, a trifluoromethyl group, a cyano group, a nitro group, or A carbonimidoyl group is intended.
  • Two electron-withdrawing groups may be bonded to each other to form a cyclic structure.
  • the term “salt” is intended to include cations such as alkali metals, alkaline earth metals, and heavy metals; organic cations such as ammonium ions and phosphonium ions.
  • azole compound examples include 5-methylbenzotriazole, 5-aminobenzotriazole, benzotriazole, 5,6-dimethylbenzoatriazole, 3-amino-1,2,4-triazole, 1,2, Examples include 4-triazole, 3,5-dimethylpyrazole, pyrazole, and imidazole.
  • the content of the azole compound is preferably 0.001 to 1.6% by mass with respect to the total mass of the polishing liquid.
  • an azole compound may be used individually by 1 type, or may use 2 or more types together. When two or more azole compounds are used in combination, the total content is preferably within the above range. Among them, it is preferable to use two or more azole compounds in combination in that a polishing liquid having the better effect of the present invention can be obtained.
  • each aspect of 2 or more types of azole compounds it is the same as that of the aspect of said azole compound.
  • a benzotriazole compound compound containing a benzotriazole skeleton
  • a compound different from the benzotriazole compound benzotriazole
  • a polishing liquid having a better effect of the present invention can be obtained.
  • a compound not containing a skeleton a compound not containing a skeleton
  • the compound that does not contain the benzotriazole skeleton is not particularly limited, but includes a 1,2,4-triazole compound, a pyrazole compound, and an imidazole compound in that a polishing liquid having a better effect of the present invention can be obtained. It is preferably at least one selected from the group.
  • the content of the anticorrosive (C) is preferably 0.001 to 1.6% by mass with respect to the total mass of the polishing liquid.
  • an anticorrosive agent (C) may be used individually by 1 type, or may use 2 or more types together. When using together 2 or more types of anticorrosives (C), it is preferable that total content is in the said range.
  • the content of the anticorrosive (C) preferably satisfies the following relationship with the content of the alcohol A. That is, the mass ratio of the content of the alcohol A to the content of the anticorrosive agent (alcohol A content / content of the anticorrosive agent; also referred to as “Alc / C” ratio) is preferably 0.004 or more, 0 .0045 or more is more preferable, 0.01 or more is further preferable, 0.03 or more is particularly preferable, 0.04 or more is most preferable, 30 or less is preferable, 25 or less is more preferable, and 5 or less is more preferable. When the Alc / C ratio is 0.01 or more, a better polishing rate can be obtained when the polishing liquid is applied to CMP.
  • the Alc / C ratio is 0.04 or more, dishing is less likely to occur on the surface to be polished of the object to be polished when the polishing liquid is applied to CMP.
  • the Alc / C ratio is 5 or less, dishing is less likely to occur on the surface of the object to be polished when the polishing liquid is supplied to CMP.
  • the polishing liquid may contain an oxidizing agent. It does not restrict
  • the oxidizing agent include hydrogen peroxide, peroxide, nitric acid, nitrate, iodate, periodate, hypochlorite, chlorite, chlorate, perchlorate, and persulfate. Examples thereof include salts, dichromates, permanganates, ozone water, silver (II) salts, and iron (III) salts, and hydrogen peroxide is more preferable.
  • An oxidizing agent may be used individually by 1 type, or may use 2 or more types together.
  • a polishing liquid having a better effect of the present invention when applied to CMP of a substrate (object to be polished) containing at least one layer selected from the group consisting of tungsten and a tungsten alloy, a polishing liquid having a better effect of the present invention can be obtained.
  • the 1st oxidizing agent When using 2 or more types of oxidizing agents together, it is preferable to use together the 1st oxidizing agent with a higher oxidation-reduction potential, and the 2nd oxidizing agent (G) with a lower oxidation-reduction potential.
  • a 1st oxidizing agent at least 1 sort (s) selected from the group which consists of hydrogen peroxide and a peroxide among the said oxidizing agents, for example is preferable, and hydrogen peroxide is more preferable.
  • the second oxidizing agent for example, among the above oxidizing agents, iron (III) salts are preferable, and at least one selected from the group consisting of iron nitrate, iron phosphate, iron sulfate, and potassium ferricyanide is more preferable. Iron nitrate (Fe (NO 3 ) 3 ) is more preferable.
  • the content of the oxidizing agent is not particularly limited, but is preferably 0.1 to 9.0% by mass with respect to the total mass of the polishing liquid.
  • the content of the oxidizing agent is 0.1% by mass or more, a more excellent polishing rate can be obtained when the polishing liquid is applied to CMP.
  • the content of the oxidizing agent is 9.0% by mass or less, dishing is less likely to occur on the surface to be polished when the polishing liquid is applied to CMP.
  • it is preferable that total content is in the said range.
  • the content of the oxidizing agent preferably satisfies the following relationship with the content of the alcohol A. That is, the mass ratio of the content of the alcohol A to the content of the oxidizing agent (the content of the alcohol A / the content of the oxidizing agent; also referred to as “Alc / D” ratio) is 0.000.5 or more. Preferably, 0.005 or more is more preferable, 0.04 or more is further preferable, 0.09 or less is preferable, and 0.07 or less is more preferable. When the Alc / D ratio is 0.005 or more, a better polishing rate can be obtained when the polishing liquid is applied to CMP.
  • the Alc / D ratio is 0.04 or more, dishing is less likely to occur on the surface to be polished of the object to be polished when the polishing liquid is applied to CMP. Further, when the Alc / D ratio is 0.07 or less, a better polishing rate can be obtained when the polishing liquid is applied to CMP.
  • the content of the second oxidizing agent preferably satisfies the following relationship with the content of the alcohol A. That is, the mass ratio of the content of the alcohol A to the content of the second oxidant (content of alcohol A / content of the second oxidant; also referred to as “Alc / G” ratio) is 0. 1 to 20 is preferable.
  • the polishing liquid may contain a charge adjusting agent.
  • the charge adjusting agent is not particularly limited, and a known charge adjusting agent can be used.
  • the charge adjusting agent has actions such as adjusting the pH of the polishing liquid to the above range and / or adjusting the ionic strength of the polishing liquid to a desired range.
  • Examples of the charge adjusting agent include acids, alkalis, and salt compounds.
  • the charge control agent is at least one selected from the group consisting of an inorganic acid, an ammonium salt of an organic acid, and an ammonium salt of an inorganic acid, in that a polishing liquid having a better effect of the present invention can be obtained. It is preferable to contain.
  • Examples of inorganic acids include sulfuric acid, hydrochloric acid, and nitric acid.
  • Examples of the organic acid ammonium salt include ammonium benzoate and ammonium citrate.
  • Examples of the inorganic acid ammonium salt include ammonium sulfate, ammonium hydrochloride, and ammonium nitrate.
  • the content of the charge control agent is not particularly limited, but is preferably 0.5 mass ppm or more, more preferably 1 mass ppm or more, still more preferably 10 mass ppm or more, based on the total mass of the polishing liquid, and 2 mass%. The following is preferable and 1200 mass ppm or less is more preferable.
  • the content of the charge adjusting agent is 10 mass ppm or more, defects are less likely to occur on the surface to be polished even when the polishing liquid is applied to CMP.
  • a charge control agent may be used individually by 1 type, or may use 2 or more types together. When two or more kinds of charge control agents are used in combination, the total content is preferably within the above range.
  • the content of the charge adjusting agent preferably satisfies the following relationship with the content of the alcohol A. That is, the mass ratio of the content of the alcohol A to the content of the charge control agent (ratio of the content of the alcohol A / the content of the charge control agent; also referred to as “Alc / E” ratio) is 0.005.
  • the above is preferable, 0.1 or more is more preferable, 500 or less is preferable, 50 or less is more preferable, and less than 5 is still more preferable.
  • the Alc / E ratio is 0.1 or more, a polishing liquid having better aging stability can be obtained, and when the polishing liquid is applied to CMP, a higher polishing rate can be obtained. Dishing is less likely to occur on the surface to be polished.
  • the Alc / E ratio is 50 or less, defects are less likely to occur on the surface to be polished even when the polishing liquid is applied to CMP. Further, when the Alc / E ratio is less than 5, more excellent effects of the present invention can be obtained.
  • the polishing liquid may contain a surfactant.
  • the surfactant has an action of reducing the contact angle of the polishing liquid with respect to the surface to be polished, and the polishing liquid tends to wet and spread on the surface to be polished.
  • the surfactant is not particularly limited, and a known surfactant selected from the group consisting of an anionic surfactant, a cationic surfactant, an amphoteric surfactant, a nonionic surfactant, and the like may be used. it can.
  • the anionic surfactant include carboxylic acid salts, sulfonic acid salts such as alkylbenzene sulfonic acids, sulfuric acid ester salts, and phosphoric acid ester salts.
  • Examples of the cationic surfactant include aliphatic amine salts, aliphatic quaternary ammonium salts, benzalkonium chloride salts, benzethonium chloride, pyridinium salts, and imidazolinium salts.
  • Examples of amphoteric surfactants include carboxybetaine type, aminocarboxylate, imidazolinium betaine, lecithin, and alkylamine oxide.
  • Examples of the nonionic surfactant include an ether type, an ether ester type, an ester type, a nitrogen-containing type, a glycol type, a fluorine type surfactant, and a silicon type surfactant.
  • the content of the surfactant is not particularly limited, but is preferably 0.00001 to 2.0% by mass, more preferably 0.0001 to 1.0% by mass with respect to the total mass of the polishing liquid, and 0.001 to 0.1 mass% is still more preferable.
  • the surfactant content is in the range of 0.0001 to 1.0% by mass, a polishing liquid having a more excellent effect of the present invention can be obtained.
  • surfactant may be used individually by 1 type, or may use 2 or more types together. When using 2 or more types of surfactant together, it is preferable that total content is in the said range.
  • the surfactant content preferably satisfies the following relationship with the content of the alcohol A. That is, the mass ratio of the content of the alcohol A to the content of the surfactant (content of alcohol A / content of surfactant; also referred to as “Alc / F” ratio) is 0.001 to 100. Is preferable, 0.002 to 80 is more preferable, and 0.005 to 50 is still more preferable. When the Alc / F ratio is within the above range, a polishing liquid having better defect performance can be obtained.
  • the polishing liquid may contain a hydrophilic polymer (hereinafter also referred to as “water-soluble polymer”).
  • hydrophilic polymers include polyglycols such as polyethylene glycol, alkyl ethers of polyglycols, polysaccharides such as polyvinyl alcohol A, polyvinyl pyrrolidone, and alginic acid, and carboxylic acid-containing polymers such as polymethacrylic acid and polyacrylic acid. , Polyacrylamide, polymethacrylamide, and polyethyleneimine.
  • Specific examples of such a hydrophilic polymer include water-soluble polymers described in JP2009-88243A, paragraphs 0042 to 0044, and JP2007-194261A, paragraph 0026.
  • the hydrophilic polymer is preferably a water-soluble polymer selected from polyacrylamide, polymethacrylamide, polyethyleneimine, and polyvinylpyrrolidone.
  • polyacrylamide or polymethacrylamide those having a hydroxyalkyl group on a nitrogen atom (for example, N- (2-hydroxyethyl) acrylamide polymer) or those having a substituent having a polyalkyleneoxy chain are preferred, and the weight average The molecular weight is more preferably 2000 to 50000.
  • polyethyleneimine those having a polyalkyleneoxy chain on the nitrogen atom are preferred, and those having a repeating unit represented by the following general formula are more preferred.
  • n a number of 2 to 200 (in the case of a mixture, the average number thereof).
  • Polyethyleneimine preferably has an HLB (Hydrophile-Lipophile Balance) value of 16 to 19.
  • the content of the hydrophilic polymer is not particularly limited, but is preferably 0.00001 to 2.0 mass%, more preferably 0.0001 to 1.0 mass%, and more preferably 0.0001 to 2.0 mass% with respect to the total mass of the polishing liquid. 1.0% by mass is more preferable, and 0.001 to 0.1% by mass is particularly preferable.
  • a hydrophilic polymer may be used individually by 1 type, or may use 2 or more types together. Further, a surfactant and a hydrophilic polymer may be used in combination. When two or more hydrophilic polymers are used in combination, the total content is preferably within the above range.
  • the polishing liquid may contain an organic solvent. It does not restrict
  • the said organic solvent is a component different from the alcohol A already demonstrated.
  • the organic solvent include ketone-based, ether-based, glycol ether-based, and amide-based solvents. More specifically, examples include acetone, methyl ethyl ketone, tetrahydrofuran, dioxane, dimethylacetamide, N-methylpyrrolidone, dimethyl sulfoxide, and acetonitrile. Of these, methyl ethyl ketone, tetrahydrofuran, dioxane, N-methylpyrrolidone and the like are more preferable.
  • the content of the organic solvent is not particularly limited, but is preferably 0.001 to 5.0% by mass, and more preferably 0.01 to 2.0% by mass with respect to the total mass of the polishing liquid.
  • the organic solvent may be used individually by 1 type, or may use 2 or more types together. When two or more organic solvents are used in combination, the total content is preferably within the above range.
  • the polishing liquid preferably contains water.
  • the water contained in the polishing liquid is not particularly limited, but ion exchange water, pure water, or the like can be used.
  • the water content is not particularly limited, but is preferably 90 to 99% by mass based on the total mass of the polishing liquid.
  • the polishing liquid may contain a chelating agent (that is, a hard water softening agent) as necessary in order to reduce adverse effects such as mixed polyvalent metal ions.
  • a chelating agent for example, a general-purpose hard water softening agent and / or an analogous compound thereof which are calcium and / or magnesium precipitation inhibitors can be used, and two or more of them may be used in combination as necessary.
  • the content of the chelating agent may be an amount sufficient to sequester metal ions such as mixed polyvalent metal ions, and is preferably 0.001 to 2.0% by mass in the total mass of the polishing liquid, for example. .
  • the method for producing the polishing liquid is not particularly limited, and a known production method can be used.
  • a manufacturing method of polishing liquid the method of mixing an abrasive grain, organic acid, and alcohol A is mentioned, for example.
  • other components such as an azole compound, an oxidizing agent, a charge adjusting agent, a surfactant agent, an organic solvent, water, and a chelating agent may be mixed.
  • the order in particular of mixing is not restrict
  • the aspect which prepares the mixture with which the abrasive grain and alcohol A were mixed previously, and adds another component with respect to the said mixture may be sufficient, and the mixture which mixed the abrasive grain and water beforehand is prepared. And the aspect which adds alcohol A and another component with respect to the said mixture may be sufficient.
  • the method for setting the alcohol A to a predetermined amount with respect to the total mass of the polishing liquid is not particularly limited. As said method, you may add so that it may become a predetermined quantity with respect to the total mass of polishing liquid, for example.
  • the mixing ratio of the raw materials is such that the total amount of alcohol A contained in the raw material is a predetermined amount with respect to the total mass of the polishing liquid. If the above is adjusted, the above polishing liquid can be produced.
  • a method for producing a polishing liquid by adding an oxidizing agent for example, hydrogen peroxide
  • an oxidizing agent for example, hydrogen peroxide
  • a polishing liquid stock solution in which components other than an oxidizing agent are mixed in advance before the polishing liquid is produced.
  • an oxidizing agent is mixed with a polishing liquid stock solution containing a predetermined component to obtain a polishing liquid. Therefore, the content of the oxidizing agent with respect to the total mass of the polishing liquid is controlled within a desired range. Cheap. This is because some oxidizing agents decompose over time and the content in the polishing liquid changes.
  • the concentrated liquid of the polishing liquid containing a predetermined component is prepared, and at least one selected from the group consisting of an oxidant and water is added to the polishing liquid.
  • a method for producing a polishing liquid having the following characteristics.
  • a chemical mechanical polishing method including a step of moving the polishing body and the polishing pad relatively to polish the surface to be polished to obtain a polished target body (hereinafter also referred to as “polishing step”). Also referred to as “CMP method”.
  • Examples of the object to be polished by the CMP method include an embodiment containing at least one layer selected from the group consisting of copper, copper alloy, tungsten, tungsten alloy, silicon nitride, and polysilicon.
  • a barrier metal film (barrier metal layer) formed on the entire surface of an interlayer insulating film (interlayer insulating layer) having a recess, and a recess is embedded in the surface of the barrier metal film.
  • a substrate is typically a semiconductor substrate, and is preferably an LSI having wiring made of copper metal and / or copper alloy, and the wiring is particularly preferably a copper alloy.
  • a semiconductor device such as a wafer in which a conductive material film is formed on a substrate, a laminate in which a conductive material film is formed on an interlayer insulating film provided on a wiring formed on the substrate, etc. Mention may be made of all stages of material that require planarization in the manufacturing process.
  • a copper alloy containing silver is preferable among the copper alloys.
  • the copper content contained in the copper alloy is preferably 40% by mass or less, more preferably 10% by mass or less, still more preferably 1% by mass or less, and in the range of 0.00001 to 0.1% by mass. Exhibits the most excellent effect on the layer.
  • the substrate examples include those used in an 8-inch or 12-inch semiconductor wafer manufacturing process or a micromachine manufacturing process.
  • the types include semiconductor silicon wafers, SOI (Silicon-On-Insulator) wafers, compound semiconductor sapphire substrates used for semiconductor lasers, and the like.
  • SOI Silicon-On-Insulator
  • compound semiconductor sapphire substrates used for semiconductor lasers, and the like.
  • the target wafer to be subjected to CMP with the polishing liquid preferably has a diameter of 200 mm or more, and particularly preferably 300 mm or more.
  • the interlayer insulating film preferably has a dielectric constant of 2.6 or less, and examples thereof include silicon nitride and polysilicon. Note that.
  • the thickness of the interlayer insulating film can be appropriately adjusted depending on the upper and lower portions of the wiring in the multilayer wiring, or between generations (nodes).
  • the barrier metal film is a film (layer) that is disposed between a conductor film (wiring) made of copper or a copper alloy provided on a semiconductor substrate and an interlayer insulating film to prevent copper diffusion.
  • the material of the barrier gold layer film is preferably a low-resistance metal material, and specifically includes at least one selected from tantalum, tantalum compounds, titanium, titanium compounds, tungsten, tungsten compounds, and ruthenium. It is preferable that TiN, TiW, Ta, TaN, W, WN, or Ru is included.
  • the thickness of the barrier metal film is preferably about 20 to 30 nm.
  • the object to be polished used in the CMP method according to the above embodiment can be manufactured by, for example, the following method.
  • an interlayer insulating film such as silicon nitride or polysilicon is laminated on a silicon substrate.
  • a concave portion (substrate exposed portion) having a predetermined pattern is formed on the surface of the interlayer insulating film by a known means such as resist layer formation or etching to form an interlayer insulating film composed of convex portions and concave portions.
  • tungsten, a tungsten compound, or the like is deposited by vapor deposition or CVD (chemical vapor deposition) as a barrier layer covering the interlayer insulating film along the surface irregularities.
  • a conductive material layer (hereinafter referred to as a conductor layer) that covers the barrier layer so as to fill the recess, and has a laminated structure.
  • a polished body is obtained.
  • the thicknesses of the interlayer insulating film, the barrier layer, and the copper body layer are preferably about 0.01 to 2.0 ⁇ m, 1 to 100 nm, and 0.01 to 2.5 ⁇ m, respectively.
  • the polishing apparatus capable of performing the CMP method is not particularly limited, and a known chemical mechanical polishing apparatus (hereinafter also referred to as “CMP apparatus”) can be used.
  • CMP apparatus for example, a holder that holds an object to be polished (for example, a semiconductor substrate) having a surface to be polished and a polishing pad to which a polishing pad is attached (a motor that can change the number of revolutions is attached).
  • a general CMP apparatus provided with a board can be used.
  • Reflexion manufactured by Applied Materials
  • polishing is preferably performed at a polishing pressure, that is, a pressure generated on the contact surface between the surface to be polished and the polishing pad of 3000 to 25000 Pa, and more preferably 6500 to 14000 Pa. .
  • the polishing is preferably performed at a rotation speed of the polishing platen of 50 to 200 rpm, more preferably 60 to 150 rpm.
  • the holder may be further rotated and / or swayed, the polishing platen may be rotated on a planetary surface, or the belt-like polishing pad may be elongated. It may be moved linearly in one direction.
  • the holder may be in a fixed, rotating, or swinging state.
  • polishing liquid supply method In the CMP method according to the above embodiment, the polishing liquid is continuously supplied to the polishing pad on the polishing surface plate by a pump or the like while the surface to be polished is polished. Although there is no restriction
  • the aspect of the polishing liquid is as described above.
  • Example 1 Each component shown below was mixed to prepare a chemical mechanical polishing liquid.
  • Colloidal silica (average primary particle size: 35 nm, product name “PL3”, manufactured by Fuso Chemical Industries, applicable to abrasive grains) 0.1% by mass ⁇ Glycine (corresponds to organic acids and amino acids) 1.5% by mass ⁇ 5-methylbenzotriazole (corresponds to azole compound containing benzotriazole skeleton) 0.001% by mass ⁇ 3-amino-1,2,4-triazole (corresponds to a compound not containing a benzotriazole skeleton and a compound containing a 1,2,4-triazole skeleton) 0.2% by mass ⁇ Hydrogen peroxide (corresponds to oxidizing agent) 1.0% by mass ⁇ Ammonium nitrate (corresponds to charge control agent) 1000 mass ppm ⁇ Methanol (corresponding to alcohol A) 500ppm ⁇ Water (pure water) remaining
  • Examples 2 to 54, Comparative Examples 1 to 5 Each component shown in Table 1, Table 2, Table 3, and Table 4 was mixed by the same method as in Example 1 to obtain each polishing liquid.
  • each abbreviation in Table 1 shows the following compounds.
  • “content” in Table 1 represents a value based on mass. The pH of each treatment solution was adjusted to the target pH by adding KOH / H 2 SO 4 .
  • PL3 Cold silica, product name “PL3”, manufactured by Fuso Chemical Industries, average primary particle size: 35 nm, corresponding to abrasive grains
  • Gly corresponds to glycine, organic acid and amino acid
  • Ala corresponds to alanine, organic acid and amino acid
  • Asp corresponds to aspartic acid, organic acid and amino acid
  • NMG corresponds to N-methylglycine, organic acid and amino acid
  • MaloA corresponds to malonic acid and organic acid
  • 5-MBTA corresponds to 5-methylbenzotriazole, azole compound containing benzotriazole skeleton
  • -BTA corresponds to benzotriazole, azole compound containing benzotriazole skeleton
  • 5,6-DMBTA corresponds to 5,6-dimethylbenzotriazole, azole compound containing benzotriazole skeleton
  • 5-ABTA corresponds to 5-aminobenzo
  • Polishing device Reflexion (manufactured by Applied Materials) ⁇ Substance to be polished (wafer): (1) For polishing speed calculation; Copper: Blanket wafer with a diameter of 300 mm on which a Cu film having a thickness of 1.5 ⁇ m is formed on a silicon substrate Tungsten: Blanket wafer with a diameter of 300 mm on which a W film with a thickness of 0.2 ⁇ m is formed on a silicon substrate Silicon nitride: thickness on a silicon substrate 300 mm diameter blanket wafer polysilicon formed with a 1.5 ⁇ m silicon nitride film: 300 mm diameter blanket wafer formed with a 1.5 ⁇ m thick polysilicon film on a silicon substrate (2) For dishing evaluation; Copper: Copper wiring wafer (pattern wafer) with a diameter of 300 mm (mask pattern 754 C
  • Polishing rate calculation The blanket wafer of (1) was polished for 60 seconds, and the metal film thickness before and after polishing was calculated from the electrical resistance value at 49 equally spaced locations on the wafer surface. The average value obtained by dividing by the value was used as the polishing rate and evaluated according to the following criteria. The results are shown in Tables 1 to 4.
  • the polishing rate is preferably C or more for practical use.
  • ⁇ Tungsten (W) polishing rate A: The polishing rate is 250 nm / min or more. B: The polishing rate is 150 nm / min or more and less than 250 nm / min. C: The polishing rate is 50 nm / min or more and less than 150 nm / min. D: The polishing rate is less than 50 nm / min.
  • SiN polishing rate A: The polishing rate is 30 nm / min or more. B: The polishing rate is 20 nm / min or more and less than 30 nm / min. C: The polishing rate is 10 nm / min or more and less than 20 nm / min. D: The polishing rate is less than 10 nm / min.
  • D Dishing is more than 25 nm and 30 nm or less.
  • E Dishing is more than 30 nm and 35 nm or less.
  • F Dishing is more than 35 nm and 40 nm or less.
  • G Dishing is more than 40 nm and 45 nm or less.
  • H Dishing is over 45 nm.
  • the polishing liquid of Example 1 contains 0.1% by mass of PL3 as abrasive grains (the same applies to the total mass of the polishing liquid), and 1.5% by mass of Gly as an organic acid.
  • As an anticorrosive agent 5-MBTA and 3-AT are contained at 0.001% by mass and 0.2% by mass, respectively, H 2 O 2 is contained at 1.0% by mass as an oxidant, and Am is used as a charge control material.
  • -Ni is contained in an amount of 1000 ppm by mass
  • MeOH as an alcohol A is contained in an amount of 500 ppm by mass
  • the balance is water.
  • the pH is 7, and the content ratio of the content of alcohol A to each component is 0.50 for abrasive grains, 0.033 for organic acids, 0.25 for anticorrosives (total), oxidation 0.050 for the agent, 0.50 for the charge preparation agent, the zeta potential is ⁇ 45 mV, the stability over time is “A”, the Cu polishing rate is 375 nm / min, and the evaluation is “B”, The dishing was 17 nm, the evaluation was “B”, and the defect performance was “A”. The same applies to Table 2 and Tables 2 to 4.
  • Example 55 In Example 1, except that ethanol was used instead of methanol, a polishing liquid according to Example 55 was prepared and evaluated in the same manner as described above. there were.
  • Example 56 In Example 1, a polishing liquid according to Example 56 was prepared in the same manner except that 1-propanol was used instead of methanol, and the same evaluation as above was performed. It was a result.
  • Example 57 In Example 1, except that isopropanol was used instead of methanol, a polishing liquid according to Example 57 was prepared and evaluated in the same manner as described above. there were.
  • Example 58 Polishing according to Example 58 in the same manner as in Example 1, except that the abrasive grains were changed from PL3 to PL2 (colloidal silica, product name “PL2”, manufactured by Fuso Chemical Industries, average primary particle size: 25 nm). A liquid was prepared and evaluated in the same manner as described above. The evaluation result was the same as in Example 1.
  • a polishing liquid for chemical mechanical polishing containing abrasive grains, organic acid, and alcohol A, where alcohol A is methanol, ethanol, 1-propanol, and isopropanol.
  • the polishing liquids of Examples 1 to 41 which are at least one selected from the group consisting of, and the content of alcohol A is 1.0 to 800 ppm by mass in the total mass of the polishing liquid, have the desired effect. Had. On the other hand, the polishing liquids of Comparative Examples 1 to 4 did not have the desired effect.
  • the polishing liquids of Examples 1, 3, and 4 in which the content ratio of alcohol A to organic acid is 0.001 to 0.05 is superior to the polishing liquid of Example 2 over time.
  • polishing liquid had a higher polishing rate and dishing performance than the polishing liquid of Example 5.
  • the polishing liquids of Examples 1, 39, and 40 in which the content of the charge adjusting agent is 10 to 1000 ppm by mass, are less defective when applied to CMP than the polishing liquid of Example 38. It was more suppressed.
  • the polishing liquid had better temporal stability than the polishing liquid of Example 37, and the occurrence of defects was further suppressed when applied to CMP.
  • polishing liquids of Examples 3, 4, 1, 5, 40, and 39 in which the content ratio of alcohol A to the charge adjusting agent is 0.1 to 50 are compared with the polishing liquid of Example 41.
  • the occurrence of defects was further suppressed.
  • the polishing liquid had better temporal stability than the polishing liquid of Example 38, and the occurrence of defects was further suppressed when applied to CMP.
  • the polishing liquids of Examples 11, 1, and 12 having a pH of 5.0 to 8.0 have superior temporal stability compared to the polishing liquid of Example 10, and CMP When applied to, the occurrence of defects was further suppressed.
  • the polishing liquid had better dishing performance than the polishing liquid of Example 13.
  • the polishing liquids of Examples 1 and 15 having an organic acid content of 1.0 to 20% by mass had a superior polishing rate compared to the polishing liquid of Example 14.
  • the polishing liquid had better dishing performance than the polishing liquid of Example 16.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)

Abstract

La présente invention vise à fournir un liquide de polissage, des grains abrasifs dans le liquide de polissage étant peu susceptibles de s'agglomérer et, même lors d'une utilisation en CMP, des défauts étant moins susceptibles de se produire dans une surface polie. La présente invention vise également à fournir un procédé de polissage chimico-mécanique. Ce liquide de polissage est utilisé pour un polissage chimico-mécanique et contient des grains abrasifs, un acide organique et de l'alcool A. L'alcool A est au moins un type choisi parmi le groupe constitué de méthanol, d'éthanol, de 1-propanol et d'isopropanol. La teneur en alcool A est comprise entre 1,0 et 800 ppm en masse de la masse totale du liquide de polissage.
PCT/JP2017/015979 2016-06-03 2017-04-21 Liquide de polissage et procédé de polissage chimico-mécanique Ceased WO2017208667A1 (fr)

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JP6652638B2 (ja) 2020-02-26
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